関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Aminothiazole | HCID 2155 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | HCID 178418790 | HCID 178418790 | — |
| 生成物 | 1-methyl-1H-pyrrole-2-ethylamine | HCID 565058 | — |
| 生成物 | HCID 178418790 | HCID 178418790 | — |
反応手順
An isothiocyanate of 2-(2-aminoethyl)-1-methylpyrrole was prepared according to Ann 657, 104-107 (1962). 1H-NMR (CDCl3) δ2.95 (t, 2H), 3.55 (s, 1H), 3.65 (t, 2H), 5.9-5.95 (m, 1H), 6.05 (t, 1H), 6.55 (t, 1H). This isothiocyanate was dissolved in DMF (4 ml). To this solution was added 200 mg (2 mmol) of 2-aminothiazole and the solution was heated at 100° C. for about 16 h. EtOAc was added and the organic phase was washed with sat. NH4Cl-solution and brine. After drying (Na2SO4), the product was purified on a silica gel column, using EtOAc/Hexane 1:1, as eluent. This gave almost pure titled product. Recrystallization from toluene/hexanes gave 150 mg of the titled product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05593993 |
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| 出典データセット | uspto-grants-1997_01 |
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| ORD ID | ord-5af45679aca346f584e32cbf4db3e202 |
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| 出典メモ | uspto-grants-1997_01 |
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